EP3975212A1 - A method for preparation of a sintered type ndfeb permanent magnet with an adjusted grain boundary - Google Patents

A method for preparation of a sintered type ndfeb permanent magnet with an adjusted grain boundary Download PDF

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Publication number
EP3975212A1
EP3975212A1 EP21199754.9A EP21199754A EP3975212A1 EP 3975212 A1 EP3975212 A1 EP 3975212A1 EP 21199754 A EP21199754 A EP 21199754A EP 3975212 A1 EP3975212 A1 EP 3975212A1
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EP
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Prior art keywords
ndfeb magnet
grain boundary
ndfeb
total amount
refers
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EP21199754.9A
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German (de)
English (en)
French (fr)
Inventor
Chuanshen Wang
Kunkun Yang
Zhongjie Peng
Kaihong Ding
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Yantai Dongxing Magnetic Materials Inc
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Yantai Shougang Magnetic Materials Inc
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
    • H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
    • H01F41/0253—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/032—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials
    • H01F1/04—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials metals or alloys
    • H01F1/047—Alloys characterised by their composition
    • H01F1/053—Alloys characterised by their composition containing rare earth metals
    • H01F1/055—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5
    • H01F1/057—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B
    • H01F1/0571—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes
    • H01F1/0575—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes pressed, sintered or bonded together
    • H01F1/0577—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes pressed, sintered or bonded together sintered
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/002—Ferrous alloys, e.g. steel alloys containing In, Mg, or other elements not provided for in one single group C22C38/001 - C22C38/60
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/005—Ferrous alloys, e.g. steel alloys containing rare earths, i.e. Sc, Y, Lanthanides
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/008—Ferrous alloys, e.g. steel alloys containing tin
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/06—Ferrous alloys, e.g. steel alloys containing aluminium
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/10—Ferrous alloys, e.g. steel alloys containing cobalt
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/12—Ferrous alloys, e.g. steel alloys containing tungsten, tantalum, molybdenum, vanadium, or niobium
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/14—Ferrous alloys, e.g. steel alloys containing titanium or zirconium
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/16—Ferrous alloys, e.g. steel alloys containing copper
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
    • H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
    • H01F41/0253—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets
    • H01F41/0266—Moulding; Pressing
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
    • H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
    • H01F41/0253—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets
    • H01F41/0293—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets diffusion of rare earth elements, e.g. Tb, Dy or Ho, into permanent magnets

Definitions

  • the invention relates to the technical field of sintered type NdFeB permanent magnets, in particular to a method for preparing sintered type NdFeB permanent magnet with an adjusted grain boundary.
  • the method may increase the coercivity of the sintered type NdFeB permanent magnet.
  • NdFeB sintered permanent magnet called "magnet kings" have been widely used since its inception and has been deeply rooted in modern society. It is widely used in high-tech fields such as electronic information, medical equipment, new energy vehicles, household appliances, robots, etc. With the rapid development of informatization and industrialization, high-performance magnets have become a current research hotspot.
  • Patent literature CN 104078176 A and JP2014209546 A show, in order to improve the coercivity, the segregation of ferromagnetic phases are suppressed in the grain boundary phase through the cooling rate forming the R6T13M phase of the La6Co11Ga13 type crystal structure.
  • Patent literature CN 108878090 reveals the high performance non-heavy rare earth NdFeB sintered permanent magnet has clear grain boundary through controlling the content of various elements and low-temperature aging.
  • Patent literature CN 105206417 A realizes the gas phase isolation of magnetic powder particles and crystal grains through the heated gasification of sulfur to make the low melting point alloy rare earth-copper aluminum. The alloy is completely separated from the main phase to obtain high coercivity.
  • Patent literature CN 102290181 A realizes a low-cost high-performance neodymium iron boron magnet without heavy rare earth or very low heavy rare earth. However, the above-mentioned magnets do not give effective method of adjustable grain boundary.
  • the present invention provides a preparation method for a sintered type NdFeB permanent magnet as defined in claim 1.
  • the method includes the steps of:
  • Figure 1 schematically shows the NdFeB magnet intermediate 3, which is composed of a NdFeB magnet 1 and a covering of a diffusion source 2.
  • the present invention proposes a method for preparing sintered type NdFeB permanent magnet with adjustable grain boundaries.
  • a NdFeB sintered permanent magnet is prepared through the synergistic effect between the elements of the magnet composition and the diffusion source, and in particular by controlling the composition ratio of the magnet composition and the diffusion source. Furthermore, clear grain boundary can improve the coercivity of NdFeB sintered permanent magnet by controlling the content of C, O, and N in the atmosphere and by argon air cooling.
  • the method for preparing sintered type NdFeB permanent magnet includes the following steps:
  • the NdFeB magnet is covered with a diffusion source to form a NdFeB magnet intermediate.
  • the chemical composition of NdFeB magnet intermediate is expressed in weight percentage as [R1 x R2 y R3 1-x-y ] a M b B c Fe 100-a-b-c , 0.8 ⁇ x ⁇ 1, 0 ⁇ y ⁇ 0.08, 32 ⁇ a ⁇ 38, 0.5 ⁇ b ⁇ 7, and 0.9 ⁇ c ⁇ 1.2.
  • R1 refers to one or more of Nd, Pr, and Ce
  • R2 refers to one or two of La and Sm
  • R3 refers to one or more of Tb, Dy, and Ho
  • M refers one or more of Al, Cu, Ga, Ti, Co, Mg, Zn, Nb, Mo, and Sn.
  • the diffusion source refers to an alloy
  • the alloying elements include one or more of Nd, Pr, Ce, La, Ho, Tb, Dy, Ga, Al, Cu, and Mg.
  • the NdFeB magnet intermediate is put into a furnace and a diffusion treatment and subsequently an aging treatment is performed.
  • the aging treatment is divided into a heating step and a cooling step.
  • the cooling step is carried out by means of argon gas positive pressure circulation cooling such that NdFeB magnets with a thickness of grain boundaries in the range of 10nm to 1 ⁇ m, preferably 30nm to 800nm, are formed.
  • a structure of the grain boundaries includes a main phase, grain boundary (a), grain boundary (b), and grain boundary (c).
  • Grain boundary (a) meets the following conditions: R ⁇ 55wt% or 35wt% ⁇ R ⁇ 40wt%, 10wt% ⁇ M ⁇ 28wt%, where 3:1 ⁇ Nd/(Pr or Ce or La) ⁇ 2:1, and (Cu+Al+Ga)/M ⁇ 0.8;
  • the grain boundary thicknesses and their compositions are measured by Zeiss EVOMA10 (SEM) Scanning Electron Microscope Measurement and EDS (Energy Dispersive Spectrometer) respectively.
  • Grain boundary (a) is the trigonometric position 1, which is in junction of the three main phases.
  • Grain boundary (b) is the two grain boundary phase position.
  • Grain boundary (c) is the trigonometric position 2, which is in junction of the three main phases.
  • the aging treatment is divided into a heating process and a cooling process.
  • Argon gas is used for the cooling process.
  • the pressure and temperature of argon gas may determine the cooling rate of magnets.
  • a temperature of argon gas may be 10°C to 20°C, preferably 15°C.
  • a pressure of the argon gas used for argon gas positive pressure circulation cooling is in the range of 1 bar to 5 bar
  • the NdFeB magnet is cooled down by the argon gas, which may pass through a (copper) tube-fin type annular exchanger. Thereby, a uniform cooling rate is achieved.
  • the pressure of the circulated argon gas is an important parameter of the process as demonstrated in below Examples 1 to 13.
  • the composition of the NdFeB magnet intermediate and the argon pressure together determine the grain boundary thickness.
  • the way of cooling using the tube-fin type annular exchanger may include vertical cooling or parallel cooling or vertical and parallel alternating cooling.
  • the temperature for diffusion treatment of the NdFeB magnet is preferably in the range of 850°C to 920°C for 6h to 20h.
  • the temperature for aging treatment is preferably in the range of 420°C to 680°C for 3h to 10h.
  • the method of covering the diffusion source on the NdFeB magnet may be any one of magnetron sputtering coating, vapor deposition coating, slurry coating, and sticking powder coating.
  • the NdFeB magnet intermediate may refer to non-heavy rare earth type intermediate or heavy rare earth type intermediate.
  • the chemical composition of the non-heavy rare earth NdFeB magnet intermediate may be [R1 x R2 1-x ] a M b B c Fe 100-a-b-c
  • the chemical composition of the non-heavy rare earth NdFeB magnet intermediate fulfils one or more of the following conditions:
  • the chemical composition of the heavy rare earth type NdFeB magnet intermediate may be [R1 x R3 y R2 1-x-y ] a M b B c Fe 100-a-b-c
  • the chemical composition of the heavy rare earth type NdFeB magnet intermediate fulfils one or more of the following conditions:
  • the content of B may preferably be 0.92 ⁇ c ⁇ 1.0.
  • the non-heavy rare earth NdFeB magnet coercivity can attain 1990 kA/m or more after high temperature and aging treatment.
  • heavy rare earth NdFeB magnet coercivity can attain 2308.4 kA/m or more after high temperature and aging treatment.
  • NdFeB magnet intermediate of specific composition is formed by a matching combination between the magnet composition and the diffusion source composition.
  • the grain boundary thickness can be controlled effectively by the diffusion temperature, the aging temperature, and the argon gas positive pressure cooling. Mass production of products can be achieved by simple experimental conditions.
  • the non-heavy rare earth NdFeB magnet coercivity can attain 1990 kA/m or more.
  • a heavy rare earth NdFeB magnet including 1.13 wt% of Tb showed a coercivity of 2308.4 kA/m.
  • the production cost is greatly reduced, and it is suitable for industrial production.
  • the method has not harsh requirements for C, O, and N and other atmosphere elements, which is easy for mass production.
  • the invention proposes that the thickness of grain boundary can be accurately controlled to achieve specific performance of the magnet by the matching combination between the magnet composition and the diffusion source composition and experimental conditions.
  • the NdFeB magnet intermediates are formed through coating NdFeB magnets with a diffusion source.
  • the examples are as followings.
  • the NdFeB magnet 1 and the diffusion source 2 form the NdFeB magnet intermediate 3, as schematically illustrated in Figure 1 .
  • Diffusion temperature, diffusion time, aging temperature, and aging time and the cooling Argon pressure with the compositon of NdFeB magnet intermediate represent suitable parameters for controlling the grain boundary thickness and thereby an increase of the performance of the NdFeB magnet could be achieved.
  • the NdFeB magnet intermediate compositions are shown in Table 1. Treatment process, rain boundary thickness and performance are displayed in Table 2.
  • the coercivity of non-heavy rare earths can be higher than 1990 kA/m, and the coercivity of magnets containing heavy rare earths after treatment can be higher than 2308.4 kA/m.
  • composition of the NdFeB magnet intermediate and the experimental conditions can effectively form different thicknesses of grain boundaries, including non-heavy rare earth NdFeB magnets and heavy rare earth NdFeB magnets.

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Power Engineering (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Hard Magnetic Materials (AREA)
  • Powder Metallurgy (AREA)
  • Manufacturing Cores, Coils, And Magnets (AREA)
EP21199754.9A 2020-09-29 2021-09-29 A method for preparation of a sintered type ndfeb permanent magnet with an adjusted grain boundary Pending EP3975212A1 (en)

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CN113871122A (zh) * 2021-09-24 2021-12-31 烟台东星磁性材料股份有限公司 低重稀土磁体及制造方法
CN115780081B (zh) * 2022-11-23 2023-07-21 中钢天源安徽智能装备股份有限公司 一种弱磁性矿用干式高梯度磁选机
CN115714054A (zh) * 2022-12-06 2023-02-24 浙江英洛华磁业有限公司 一种含Mg的高性能钕铁硼磁体及其制备方法

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JP7409754B2 (ja) 2024-01-09
JP2023022014A (ja) 2023-02-14
US20220102034A1 (en) 2022-03-31
CN112133552B (zh) 2022-05-24
JP2022056372A (ja) 2022-04-08
CN112133552A (zh) 2020-12-25

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